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Nanocomposites based on the poly(N-vinylcaprolactam) (PVCL) fabricated from PVCL solutions at different drying temperatures (PVCL25 at 25 °C, PVCL40 at 40 °C) and titanium oxides(IV) nanoparticles (TNPs) were produced for the first time by dry mixing and grinding and mechanical milling in a planetary ball mill using different PVCL:TNP ratios. New effects in initial PVCL (hydration) and TNP [decomposition of η-phase; appearance of hydrated titanium dioxide (HTD)] samples, as well as in PVCL [(de)hydration, disordering of the heterocycles] and TNP (amorphization, dehydration of η-phase, partial crystallization of Hombifine N with anatase), involved as components in PVCL/TNP nanocomposites, were found. The different role of each type of treatments and its conditions in the specific of the effects observed was shown. Only high-frequency mechanical milling leads to the appearance of HTD and the complete disappearance of the second peak of PVCL (disordering of the heterocycles) in PVCL/TNP nanocomposites.

Titania nanoparticles (anatase or anatase + rutile) with enhanced photocatalytic activity were successfully produced by treating titanyl sulfate with various peroxo compounds (hydrogen peroxide, ammonium persulfate, and urea hydrogen peroxide) with further annealing. Transformation of titanyl sulfate to titanium dioxide was investigated by X-ray diffraction, electron microscopy, X-ray microanalysis, IR, Raman, X-ray photoelectron, and UV/vis spectroscopy. The peroxo compound and annealing temperature play an important role in phase composition and properties of the samples. Correlations between phase composition, oxygen content, band gaps, and constant rates for methyl orange (MO) discoloration were found. The [TiOx(O2)2−x(H2O)m] phase, which forms on the first stage of the reaction, contains nanoparticles with small crystallites (1–2 nm) and promotes formation of titanium dioxide with the anatase structure. Thermal decomposition of the peroxo-containing phase results in formation of titanium dioxide. Oxygen excess prevents transformation of anatase to rutile, decreases band gap, and increases activity of titanium dioxide (anatase or anatase + rutile) in the model reaction of MO destruction.

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